CN109337687A - A kind of erbium ion sensitization up-conversion phosphor and the preparation method and application thereof - Google Patents
A kind of erbium ion sensitization up-conversion phosphor and the preparation method and application thereof Download PDFInfo
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- CN109337687A CN109337687A CN201811171699.2A CN201811171699A CN109337687A CN 109337687 A CN109337687 A CN 109337687A CN 201811171699 A CN201811171699 A CN 201811171699A CN 109337687 A CN109337687 A CN 109337687A
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Abstract
The invention belongs to luminescent material technical fields, and in particular to a kind of erbium ion sensitization up-conversion phosphor and the preparation method and application thereof.The up-conversion phosphor is with NaLuF4For matrix, with Tm3+And Ho3For energy capture center, with Er3+For sensitized ions and active ions.Wherein, pass through highly doped Er3+Mode, by Er3+It is used as sensitized ions and active ions, available high-purity red up-conversion luminescence simultaneously.By Tm3+And Ho3+It is used as energy capture center simultaneously, Er can be reduced3+Doping concentration, so that the occurrence probability of concentration quenching be effectively reduced, it is easier to realize the red up-conversion luminescence of high-purity, high intensity and high red green ratio.The up-conversion fluorescence powder preparation technique is simple, and the period is short, and equipment cost is low, easily operated, pollution-free, is suitble to large-scale production.Gained up-conversion phosphor shows etc. that fields have broad application prospects in bio-imaging, solar battery, solid state laser, device.
Description
Technical field
The invention belongs to luminescent material technical fields, and in particular to a kind of erbium ion sensitization up-conversion phosphor and its preparation
Method and application.
Background technique
Up-conversion luminescence refers to that wavelength of transmitted light is less than the luminescence phenomenon of excitation wavelength, at present predominantly rear-earth-dopedization
Close object.Rear-earth-doped up-conversion luminescent material is with fluorescence lifetime is long, bio-toxicity is low, chemical stability is high, photostability is strong
The advantages that, have wide practical use in fields such as solid state laser, solar battery, bio-imagings.Especially in bio-imaging
Field, it is main at present using depth penetrates and the 980nm exciting light of tissue damage can be reduced exciting upconverting fluorescent material.
But under this exciting light, up-conversion typically exhibits multiple emission peaks.Up-conversion is set to be preferably applied for biology
Aspect must just make its emission peak fall into biological tissue's absorption (scattering) is small, transmitance is high " optical window " (red as much as possible
Optical band (600-700nm) and near infrared band (700-1100nm)) in range.Traditional up-conversion is all with Yb3+Make
For sensitized ions, but the combined up-conversion of this doping is easy to generation fluorescent quenching, and luminous intensity is low, and is difficult to send out
Project single feux rouges.Therefore, how to develop a kind of up-conversion with high-intensitive, single red emission becomes current hair
The a great problem of luminescent material technical field.
In addition, solar battery is preferable to the assimilation effect of visible light but weaker to the absorption of near infrared light at present, therefore
If the rear-earth-doped up-conversion of high-intensitive, single red emission can be obtained, visible feux rouges is converted by near infrared light, it will
The transfer efficiency of solar battery is greatly improved.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art, the primary purpose of the present invention is that providing in a kind of sensitization of erbium ion
Conversion phosphor.The up-conversion phosphor can get the characteristic of high-intensitive, single red emission using dual energy capture center, can
Solve the problems, such as that the existing up-conversion impure and intensity that shines is inadequate.
Another object of the present invention is to provide the preparation methods of above-mentioned erbium ion sensitization up-conversion phosphor.
A further object of the present invention is to provide above-mentioned erbium ion sensitization up-conversion phosphor solar battery, biology at
The application of picture and solid state laser field.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of erbium ion sensitization up-conversion phosphor, chemical expression NaLuF4: Er/Ho/xTm, wherein NaLuF4
For matrix, Er3+For sensitized ions and active ions, Ho3+And Tm3+For energy capture center, molar ratio Lu:Er:Ho:Tm=
5:(4.95-x): 0.05:x, x=0.1~0.5.
The x is preferably equal to 0.2.At this point, up-conversion phosphor has the single red emission of the highest 660nm of intensity.
The present invention further provides the preparation methods of above-mentioned erbium ion sensitization up-conversion phosphor, comprising the following steps: will
Citric acid solution, sodium hydroxide solution and water are uniformly mixed, and lutecium nitrate solution, Nitrate Solution, holmium nitrate solution and nitre is added
Sour thulium solution is uniformly mixed, and Fluorinse and water is then added, and is uniformly mixed, and forms turbid solution, turbid solution is carried out hydro-thermal
Reaction, then the turbid solution after reaction is centrifuged, white precipitate is obtained, white precipitate is washed, is dried to get the erbium ion
It is sensitized up-conversion phosphor.
The concentration of the citric acid solution is preferably 1~3molL-1, more preferably 2molL-1。
The concentration of the sodium hydroxide solution is preferably 3~5molL-1, more preferably 4molL-1。
It is further preferred that citric acid is molten when described that citric acid solution, sodium hydroxide solution and water is uniformly mixed
The volume ratio of liquid, sodium hydroxide solution and water is 1.5:1.25:10.
Wherein, citric acid is used to adjust the pH value of solution as chelating agent, sodium hydroxide.
The preparation method preferably general of the lutecium nitrate solution, Nitrate Solution, holmium nitrate solution or thulium nitrate solution
Luteium oxide (99.99%), erbium oxide (99.99%), holimium oxide (99.99%) or thulium oxide (99.99%) are dissolved in mass fraction
For in 30% dust technology to obtain the final product.
The concentration of the lutecium nitrate solution is preferably 1molL-1。
The concentration of the Nitrate Solution is preferably 1molL-1。
The concentration of the holmium nitrate solution is preferably 0.1molL-1。
The concentration of the thulium nitrate solution is preferably 0.1molL-1。
It is further preferred that described lutecium nitrate solution, Nitrate Solution, holmium nitrate solution and the thulium nitrate solution of being added
Volume ratio is Lu:Er:Ho:Tm=5:y:0.5:x, wherein x=1~5, y=4.45~4.85.
The concentration of the Fluorinse is preferably 1molL-1。
It is further preferred that it is described be added lutecium nitrate solution, holmium nitrate solution volume and be added Fluorinse and
The volume ratio of water is 1:0.1:20:12.
The water is preferably deionized water.
The turbid solution is milky.
The condition of the hydro-thermal reaction preferably reacts 10h at 200 DEG C.
The hydro-thermal reaction container is preferably stainless steel cauldron.
The mother liquor of turbid solution after the reaction is clarified, and white precipitate is arranged at bottom.
The condition of the centrifugation is preferably centrifuged 10min under 10000 revs/min, is centrifuged altogether twice.
The mode of the washing preferably successively uses deionized water and ethanol wash.
The mode of the drying preferably dries 12h at 60 DEG C.
The present invention further provides above-mentioned erbium ion sensitization up-conversion phosphors in solar battery, bio-imaging and solid
The application of field of lasers.For example, existing solar battery is stronger in the absorption of visible light wave range, but near infrared band
Absorption is weaker, and erbium ion sensitization up-conversion phosphor efficiently can convert visible feux rouges near infrared light, favorably
In the transfer efficiency for improving solar battery.
Compared with prior art, the present invention having the following advantages and benefits:
(1) up-conversion phosphor prepared by the present invention is by Er3+It is used as sensitized ions and active ions simultaneously, by Tm3+And Ho3 +It is used as energy capture center simultaneously, can get high-intensitive, single red emission under 980nm excitation.Wherein, by highly doped
Er3+Mode, by Er3+It is used as sensitized ions and active ions, available high-purity red up-conversion luminescence simultaneously.By Tm3+
And Ho3+It is used as energy capture center simultaneously, Er can be greatly improved3+660nm red Up-conversion Intensity.Relative to list
One Tm3+Or Ho3+Energy capture center, due to Tm3+And Ho3+It is all efficient upper switch active ion, and can be as efficient
Energy capture center therefore using dual energy capture center, can realize high-purity, high-intensitive red up-conversion luminescence
While, reduce Er3+Doping concentration be easier to realize high-purity, height so that the occurrence probability of concentration quenching be effectively reduced
Intensity red up-conversion luminescence, and its is red green than up to 187.
(2) hydrogen-oxygen is used using citric acid as chelating agent in the preparation method of erbium ion sensitization up-conversion phosphor of the present invention
Change sodium and adjust solution ph, by adjusting the proportion of Lu ion, Er ion, Ho ion and Tm ion in solution, in hydro-thermal reaction
The erbium ion sensitization up-conversion phosphor of high-intensitive, the single red emission can be prepared down.The preparation process is simple,
Equipment cost is low, easy to operate, non-environmental-pollution, short preparation period, is suitble to produce in enormous quantities.
(3) up-conversion phosphor prepared by the present invention can be used for bio-imaging field, also can be by absorbing near infrared light simultaneously
Emit high-intensitive, the visible single feux rouges of 660nm and is used for the fields such as solar battery, solid state laser.
Detailed description of the invention
Fig. 1 is the fluorogram of the up-conversion phosphor of Examples 1 to 3 preparation.
Fig. 2 is the energy level transition figure of the up-conversion phosphor of Examples 1 to 3 preparation, wherein figure (a) is Er3+Sensitization, Tm3 +For the energy level transition figure at energy capture center;Scheming (b) is Er3+Sensitization, Ho3+For the energy level transition figure at energy capture center.
Fig. 3 is the X-ray diffractogram of up-conversion phosphor prepared by embodiment 2.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.For not specifically specified technological parameter, routine techniques progress can refer to.
Embodiment 1
The present embodiment provides a kind of erbium ion sensitization up-conversion phosphors and preparation method thereof.
It is 2molL by 1.5mL concentration-1Citric acid solution, 1.25mL concentration be 4molL-1Sodium hydroxide solution
It mixes, stirs 10 minutes with 10mL deionized water, sequentially adding 0.5mL concentration is 1molL-1Lutecium nitrate solution, 0.485mL
Concentration is 1molL-1Nitrate Solution, 0.05mL concentration be 0.1molL-1Holmium nitrate solution and 0.1mL concentration be
0.1mol·L-1Thulium nitrate solution, stir 30 minutes, add 10mL concentration be 1molL-1Fluorinse and 6mL
Deionized water stirs 30 minutes, forms milky turbidity liquid.Turbid solution is gone in the white bushing of stainless steel cauldron, it is close
It is honored as a queen and is put into baking oven, hydro-thermal reaction 10 hours at 200 DEG C.Turbid solution after reaction is centrifugated twice, every time
10000 revs/min of revolving speed, duration 10 minutes, obtain white precipitate.White precipitate is successively used into deionized water and ethanol wash,
It is dried at 60 DEG C 12 hours and is sensitized up-conversion phosphor to get the erbium ion.
Fluorescence intensity of the up-conversion phosphor under the excitation of 980nm near infrared light is analyzed simultaneously using fluorescence analyser
Describe its energy level transition figure, fluorogram and energy level transition figure difference are as illustrated in fig. 1 and 2, it is seen that the up-conversion phosphor exists
The excitation of 980nm near infrared light is lower can to launch high-intensitive single feux rouges.
Embodiment 2
The present embodiment provides a kind of erbium ion sensitization up-conversion phosphors and preparation method thereof.
It is 2molL by 1.5mL concentration-1Citric acid solution, 1.25mL concentration be 4molL-1Sodium hydroxide solution
It mixes, stirs 10 minutes with 10mL deionized water, sequentially adding 0.5mL concentration is 1molL-1Lutecium nitrate solution, 0.475mL
Concentration is 1molL-1Nitrate Solution, 0.05mL concentration be 0.1molL-1Holmium nitrate solution and 0.2mL concentration be
0.1mol·L-1Thulium nitrate solution, stir 30 minutes, add 10mL concentration be 1molL-1Fluorinse and 6mL
Deionized water stirs 30 minutes, forms milky turbidity liquid.Turbid solution is gone in the white bushing of stainless steel cauldron, it is close
It is honored as a queen and is put into baking oven, hydro-thermal reaction 10 hours at 200 DEG C.Turbid solution after reaction is centrifugated twice, every time
10000 revs/min of revolving speed, duration 10 minutes, obtain white precipitate.White precipitate is successively used into deionized water and ethanol wash,
It is dried at 60 DEG C 12 hours and is sensitized up-conversion phosphor to get the erbium ion.
Analysis of components is carried out to gained up-conversion phosphor using XRD, as a result as shown in Figure 3, it was demonstrated that gained fluorescence
The crystal form and hexagonal NaLuF of powder4It coincide.Up-conversion phosphor is excited in 980nm near infrared light using fluorescence analyser
Under fluorescence intensity analyzed and describe its energy level transition figure, as illustrated in fig. 1 and 2, it is seen that the up-conversion phosphor is in 980nm
Near infrared light excitation is lower can to launch high-intensitive single feux rouges.
Embodiment 3
The present embodiment provides a kind of erbium ion sensitization up-conversion phosphors and preparation method thereof.
It is 2molL by 1.5mL concentration-1Citric acid solution, 1.25mL concentration be 4molL-1Sodium hydroxide solution
It mixes, stirs 10 minutes with 10mL deionized water, sequentially adding 0.5mL concentration is 1molL-1Lutecium nitrate solution, 0.445mL
Concentration is 1molL-1Nitrate Solution, 0.05mL concentration be 0.1molL-1Holmium nitrate solution and 0.5mL concentration be
0.1mol·L-1Thulium nitrate solution, stir 30 minutes, add 10mL concentration be 1molL-1Fluorinse and 6mL
Deionized water stirs 30 minutes, forms milky turbidity liquid.Turbid solution is gone in the white bushing of stainless steel cauldron, it is close
It is honored as a queen and is put into baking oven, hydro-thermal reaction 10 hours at 200 DEG C.Turbid solution after reaction is centrifugated twice, every time
10000 revs/min of revolving speed, duration 10 minutes, obtain white precipitate.White precipitate is successively used into deionized water and ethanol wash,
It is dried at 60 DEG C 12 hours and is sensitized up-conversion phosphor to get the erbium ion.
Fluorescence intensity of the up-conversion phosphor under the excitation of 980nm near infrared light is analyzed simultaneously using fluorescence analyser
Describe its energy level transition figure, as illustrated in fig. 1 and 2.It will be seen from figure 1 that the up-conversion phosphor of Examples 1 to 3 preparation
Launch the high-purity feux rouges that wavelength is 660nm, and the up-conversion phosphor prepared in embodiment 2 has highest red emission
Intensity, it is red green than up to 187.From the figure (a) and figure (b) in Fig. 2 as can be seen that up-conversion fluorescence prepared by Examples 1 to 3
Powder is with Er3+As sensitized ions, that is, pass through Er3+Efficient absorption 980nm near-infrared excitation light, and with Tm3+And Ho3+As double
Energy capture center can get high-intensitive, high-purity red up-conversion luminescence.
Embodiment 4
The present embodiment provides a kind of erbium ion sensitization up-conversion phosphors and preparation method thereof.
It is 1molL by 1.5mL concentration-1Citric acid solution, 1.25mL concentration be 3molL-1Sodium hydroxide solution
It mixes, stirs 10 minutes with 10mL deionized water, sequentially adding 0.5mL concentration is 1molL-1Lutecium nitrate solution, 0.445mL
Concentration is 1molL-1Nitrate Solution, 0.05mL concentration be 0.1molL-1Holmium nitrate solution and 0.5mL concentration be
0.1mol·L-1Thulium nitrate solution, stir 30 minutes, add 10mL concentration be 1molL-1Fluorinse and 6mL
Deionized water stirs 30 minutes, forms milky turbidity liquid.Turbid solution is gone in the white bushing of stainless steel cauldron, it is close
It is honored as a queen and is put into baking oven, hydro-thermal reaction 10 hours at 200 DEG C.Turbid solution after reaction is centrifugated twice, every time
10000 revs/min of revolving speed, duration 10 minutes, obtain white precipitate.White precipitate is successively used into deionized water and ethanol wash,
It is dried at 60 DEG C 12 hours and is sensitized up-conversion phosphor to get the erbium ion.
Embodiment 5
The present embodiment provides a kind of erbium ion sensitization up-conversion phosphors and preparation method thereof.
It is 3molL by 1.5mL concentration-1Citric acid solution, 1.25mL concentration be 5molL-1Sodium hydroxide solution
It mixes, stirs 10 minutes with 10mL deionized water, sequentially adding 0.5mL concentration is 1molL-1Lutecium nitrate solution, 0.445mL
Concentration is 1molL-1Nitrate Solution, 0.05mL concentration be 0.1molL-1Holmium nitrate solution and 0.5mL concentration be
0.1mol·L-1Thulium nitrate solution, stir 30 minutes, add 10mL concentration be 1molL-1Fluorinse and 6mL
Deionized water stirs 30 minutes, forms milky turbidity liquid.Turbid solution is gone in the white bushing of stainless steel cauldron, it is close
It is honored as a queen and is put into baking oven, hydro-thermal reaction 10 hours at 200 DEG C.Turbid solution after reaction is centrifugated twice, every time
10000 revs/min of revolving speed, duration 10 minutes, obtain white precipitate.White precipitate is successively used into deionized water and ethanol wash,
It is dried at 60 DEG C 12 hours and is sensitized up-conversion phosphor to get the erbium ion.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of erbium ion is sensitized up-conversion phosphor, it is characterised in that: chemical expression NaLuF4: Er/Ho/xTm, wherein
NaLuF4For matrix, Tm3+And Ho3+For energy capture center, Er3+For sensitized ions and active ions, molar ratio Lu:Er:
Ho:Tm=5:(4.95-x): 0.05:x, x=0.1~0.5.
2. erbium ion according to claim 1 is sensitized up-conversion phosphor, it is characterised in that: the x=0.2.
3. the preparation method of erbium ion sensitization up-conversion phosphor of any of claims 1 or 2, which is characterized in that including following
Step: citric acid solution, sodium hydroxide solution and water are uniformly mixed, and it is molten that lutecium nitrate solution, Nitrate Solution, holmium nitrate is added
Liquid and thulium nitrate solution are uniformly mixed, and Fluorinse and water is then added, and are uniformly mixed, and turbid solution is formed, by turbid solution into
Row hydro-thermal reaction, then the turbid solution after reaction is centrifuged, white precipitate is obtained, white precipitate is washed, is dried to get described
Erbium ion is sensitized up-conversion phosphor.
4. the preparation method of erbium ion sensitization up-conversion phosphor according to claim 3, it is characterised in that:
The concentration of the lutecium nitrate solution is 1molL-1;
The concentration of the Nitrate Solution is 1molL-1;
The concentration of the holmium nitrate solution is 0.1molL-1;
The concentration of the thulium nitrate solution is 0.1molL-1。
5. the preparation method of erbium ion sensitization up-conversion phosphor according to claim 4, it is characterised in that: described adds
The volume ratio for entering lutecium nitrate solution, Nitrate Solution, holmium nitrate solution and thulium nitrate solution is Lu:Er:Ho:Tm=5:y:0.5:
X, wherein x=1~5, y=4.45~4.85.
6. the preparation method of erbium ion sensitization up-conversion phosphor according to claim 4, it is characterised in that:
The concentration of the Fluorinse is 1molL-1;
Be added lutecium nitrate solution, the volume of holmium nitrate solution and the addition Fluorinse and the volume ratio of water is 1:0.1:
20:12。
7. the preparation method of erbium ion sensitization up-conversion phosphor according to claim 3, it is characterised in that:
The concentration of the citric acid solution is 1~3molL-1;
The concentration of the sodium hydroxide solution is 3~5molL-1。
8. the preparation method of erbium ion sensitization up-conversion phosphor according to claim 7, it is characterised in that:
The concentration of the citric acid solution is 2molL-1;
The concentration of the sodium hydroxide solution is 4molL-1;
It is described when being uniformly mixed citric acid solution, sodium hydroxide solution and water, citric acid solution, sodium hydroxide solution and water
Volume ratio be 1.5:1.25:10.
9. according to the preparation method of the described in any item erbium ion sensitization up-conversion phosphors of claim 3~8, feature exists
In: the condition of the hydro-thermal reaction is to react 10h at 200 DEG C.
10. the application of erbium ion of any of claims 1 or 2 sensitization up-conversion phosphor, it is characterised in that: by the erbium from
Son sensitization up-conversion phosphor is used for solar battery, bio-imaging and solid state laser field.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115340872A (en) * | 2022-08-02 | 2022-11-15 | 广州大学 | Up-conversion fluorescent powder doped by low-concentration sensitized ions and preparation method thereof |
CN115368896A (en) * | 2022-08-02 | 2022-11-22 | 广州大学 | Low-concentration erbium ion doped strong red light up-conversion fluorescent powder and preparation method thereof |
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2018
- 2018-10-09 CN CN201811171699.2A patent/CN109337687B/en active Active
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EMORY M. CHAN ET AL.: "Combinatorial Discovery of Lanthanide-Doped Nanocrystals with Spectrally Pure Upconverted Emission", 《NANO LETTERS》 * |
HAO LIN ET AL.: "Morphology evolution and pure red upconversion mechanism of β-NaLuF4 crystals", 《SCIENTIFIC REPORTS》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115340872A (en) * | 2022-08-02 | 2022-11-15 | 广州大学 | Up-conversion fluorescent powder doped by low-concentration sensitized ions and preparation method thereof |
CN115368896A (en) * | 2022-08-02 | 2022-11-22 | 广州大学 | Low-concentration erbium ion doped strong red light up-conversion fluorescent powder and preparation method thereof |
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